CN112362766A - System for detecting gas components in sulfur hexafluoride electrical equipment - Google Patents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
Abstract
The invention discloses a system for detecting gas components in sulfur hexafluoride electrical equipment, which comprises: a sulfur chemiluminescence detection unit and a pulsed discharge helium ionization detection unit, wherein: the sulfur chemiluminescence monitoring unit comprises: the device comprises a primary diluting device 1, a current limiter 2, a quantitative ring 3, a six-way valve 4, a split/non-split sample inlet 5, a chromatographic column 6, a four-way valve 7 and a sulfur chemiluminescence detector 8; the pulse discharge helium ionization detection unit comprises a quantitative ring 9, a quantitative ring 10, a ten-way valve 11, a chromatographic column 12, a chromatographic column 14, a chromatographic column 15, a four-way valve 13, a four-way valve 16 and a pulse discharge helium ionization detector 17. The embodiment of the invention combines a sulfur chemiluminescence detector and a pulse discharge helium ionization detector, the sulfur chemiluminescence detector has equimolar linear response to the response of sulfur-containing compounds, the sensitivity is high, the linearity is wide, the linear range of the response of the pulse discharge helium ionization detector to organic matters is as high as 105, and the minimum detection limit can be as low as ppb level.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a system for detecting gas components in sulfur hexafluoride electrical equipment.
Background
Sulfur hexafluoride (SF)6) Gases are widely used in high voltage electrical equipment due to their excellent insulating and arc extinguishing properties, but SF6In the presence of discharge, ions and radicals are decomposed and formed, and after the discharge is completed, most of them are recombined into SF6But some of them produce harmful sulfur tetrafluoride (SF)4) Sulfur difluoride (SF)2) And the like. When moisture and oxygen are present inside the apparatus, the subfluorides chemically react with these components to form a variety of oxygen-containing fluorosulfides such as sulfur dioxide (SO)2) Thionyl fluoride (SOF)2) Sulfuryl fluoride (SO)2F2) Hydrogen sulfide (H)2S), carbonyl sulfide (COS), carbon disulfide (CS)2) And the like. In addition, the relevant standards specify the use of carbon tetrafluoride (CF) for air4) And detecting the fluorocarbon compound. The detection methods commonly used for these components at present mainly include: detection tube method, infrared absorption spectrometry, gas chromatography-mass spectrometry, electrochemical sensor method, ultraviolet absorption spectrometry, mass spectrometry, ion mobility spectrometry, and photoacoustic spectrometrySpectrum, etc. The detection tube method can only detect SO2HF and H2S and the like, and the detection result is not high in precision and is easily influenced by the temperature and the humidity of the environment. The infrared absorption spectroscopy has the disadvantages that the infrared absorption spectra of different gas components may partially overlap, absorption peaks thereof interfere with each other, the difficulty of quantitative analysis is greatly increased, and the equipment cost is high. The disadvantage of the electrochemical sensor method is that the products that can be identified are currently limited to SO2、HF、H2S and CO, and the decomposition products can cause misjudgment due to signal cross interference, and in addition, the service life of part of the sensors is short and the price is high. The defects of the ion mobility chromatography are poor resolution and narrow linear range. The mass spectrometry has the defects of high equipment cost, complex maintenance and unsuitability for large-scale popularization. The ultraviolet absorption spectrometry has the defect that SO is contained2F2、SOF2The absorption of various important derivatives in the organic electroluminescent material is concentrated in the vacuum ultraviolet region (about 150-200 nm), and O2The derivative has strong absorption in the region, and the types of the derivative suitable for detection in the region of more than 200nm are very limited, so that the application of ultraviolet absorption spectroscopy is restricted. The photoacoustic spectroscopy has the disadvantages of being greatly affected by the ambient temperature and having the problem of cross interference of different derivatives. The gas chromatography uses a chromatographic column to separate different components to be detected, and combines a high-sensitivity detector to realize quantitative detection of each component, which is currently the most commonly used SF6Laboratory test method for decomposition products. The gas chromatography has the outstanding advantages of multiple detection components, high sensitivity, accurate quantification and the like. The commonly used detectors of the gas chromatograph mainly comprise a hydrogen flame detector, a thermal conductivity detector, a flame photometric detector, a pulse discharge helium ionization detector and a sulfur chemiluminescence detector. The hydrogen flame detector does not respond to inorganic substances such as air and the like, needs three gas sources and is destructive to a detected sample; the thermal conductivity detector has low sensitivity, and when the flame photometric detector detects sulfur-containing components, the flame photometric detector is nonlinear and cannot accurately and quantitatively detect the sulfur-containing components.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a system for detecting gas components in sulfur hexafluoride electrical equipment.
In order to solve the above problems, the present invention provides a system for detecting a gas component in sulfur hexafluoride electrical equipment, the system including: a sulfur chemiluminescence detection unit and a pulsed discharge helium ionization detection unit, wherein:
the sulfur chemiluminescence monitoring unit comprises: the device comprises a primary diluting device 1, a current limiter 2, a quantitative ring 3, a six-way valve 4, a split/non-split sample inlet 5, a chromatographic column 6, a four-way valve 7 and a sulfur chemiluminescence detector 8;
the pulse discharge helium ionization detection unit comprises a quantitative ring 9, a quantitative ring 10, a ten-way valve 11, a chromatographic column 12, a chromatographic column 14, a chromatographic column 15, a four-way valve 13, a four-way valve 16 and a pulse discharge helium ionization detector 17;
the primary diluting device 1 is connected with the six-way valve 4, the current limiter 2, the ten-way valve 11, the pulse discharge helium ionization detector 17 and the four-way valve 13 through gas circuits;
the flow restrictor 2 is connected with the four-way valve 7, the primary diluting device 1, the flow restrictor 2, the ten-way valve 11, the pulse discharge helium ionization detector 17 and the four-way valve 13 through gas circuits;
the quantitative ring 3 is connected to the six-way valve 4 through a gas path;
the flow dividing/non-flow dividing sample inlet 5 is connected with the four-way valve 7 and the chromatographic column 6 through a gas circuit;
the chromatographic column 6 is connected with the four-way valve 7 through a gas circuit, and the sulfur chemiluminescence detector 8 is connected with the four-way valve 7 through a gas circuit;
the chromatographic column 12 is connected with the ten-way valve 11 and the four-way valve 13 through gas circuits;
the chromatographic column 15 is connected with the ten-way valve 11 and the four-way valve 16 through gas circuits;
the chromatographic column 14 is connected with the four-way valve 13 and the four-way valve 16 through gas circuits;
the pulse discharge helium ionization detector 17 is connected with the four-way valve 16, the primary diluting device 1, the current limiter 2, the six-way valve 4 and the ten-way valve 11 through gas circuits.
The first-stage diluting device 1 is connected with the six-way valve 4 based on a three-way joint.
The four-way valve 13 is also connected with a pre-separation column based on a gas circuit.
The primary diluting device consists of an EPC control system, an air capillary column of 0.32mm multiplied by 30m, a capillary tee joint and a gas circuit connecting system and is used for diluting a gas sample.
The quantitative ring 3 is a quantitative ring which has the volume of 0.25mL and is treated by a passivation process.
The chromatographic column 6 adopts a DB-sulfurur-SCD capillary column or a Gaspro capillary column and is used for separating sulfur-containing gas components in sulfur hexafluoride electrical equipment.
The volume of the quantitative ring 9 and the quantitative ring 10 is 1mL, and the ten-way valve 11 is used for respectively conveying the gas samples in the two quantitative rings to a chromatographic column separation system.
The chromatographic column 12 adopts a CST pre-separation column, the chromatographic column 14 adopts a 13X packed column, and the chromatographic column 15 adopts a PQ packed column.
In an embodiment of the invention, a combination of a Sulfur Chemiluminescence Detector (SCD) with a Pulsed Discharge Helium Ionization Detector (PDHID) having an equimolar linear response to the response of sulfur-containing compounds, high sensitivity (< 0.5pg S/sec), and broad linearity (> 1X 10)-4) The sulfur chemiluminescence detection unit can detect sulfuryl fluoride (SO) in sulfur hexafluoride without the interference of most sample matrixes and quenching effect and the like2F2) Thionyl fluoride (SOF)2) Hydrogen sulfide (H)2S), sulfur dioxide (SO)2) Carbonyl sulfide (COS), carbon disulfide (CS)2) The gas components are equal; a Pulse Discharge Helium Ionization Detector (PDHID) is a high-sensitivity nondestructive detector with a response linear range of 10 to organic substances5The minimum detection limit can be as low as ppb level.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a system for detecting a gas component in sulfur hexafluoride electrical equipment in an embodiment of the present invention;
FIG. 2 is a SO in an embodiment of the present invention2F2、SOF2、H2S、SO2A chromatogram peak profile of;
FIG. 3 is a COS chromatogram peak plot in an example of the present invention;
FIG. 4 is a CS in an embodiment of the present invention2Chromatogram peak images;
FIG. 5 is a drawing H in an embodiment of the present invention2、O2、N2、CO、CH4、CF4、CO2、C2F6、C3F8Peak of chromatogram.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a system for detecting gas components in sulfur hexafluoride electrical equipment in an embodiment of the present invention, where the system includes: a sulfur chemiluminescence detection unit and a pulsed discharge helium ionization detection unit, wherein:
the sulfur chemiluminescence monitoring unit comprises: the device comprises a primary diluting device 1, a current limiter 2, a quantitative ring 3, a six-way valve 4, a split/non-split sample inlet 5, a chromatographic column 6, a four-way valve 7 and a sulfur chemiluminescence detector 8; the pulse discharge helium ionization detection unit comprises a quantitative ring 9, a quantitative ring 10, a ten-way valve 11, a chromatographic column 12, a chromatographic column 14, a chromatographic column 15, a four-way valve 13, a four-way valve 16 and a pulse discharge helium ionization detector 17; the primary diluting device 1 is connected with the six-way valve 4, the current limiter 2, the ten-way valve 11, the pulse discharge helium ionization detector 17 and the four-way valve 13 through gas circuits; the flow restrictor 2 is connected with the four-way valve 7, the primary diluting device 1, the flow restrictor 2, the ten-way valve 11, the pulse discharge helium ionization detector 17 and the four-way valve 13 through gas circuits; the quantitative ring 3 is connected to the six-way valve 4 through a gas path; the flow dividing/non-flow dividing sample inlet 5 is connected with the four-way valve 7 and the chromatographic column 6 through a gas circuit; the chromatographic column 6 is connected with the four-way valve 7 through a gas circuit, and the sulfur chemiluminescence detector 8 is connected with the four-way valve 7 through a gas circuit; the chromatographic column 12 is connected with the ten-way valve 11 and the four-way valve 13 through gas circuits; the chromatographic column 15 is connected with the ten-way valve 11 and the four-way valve 16 through gas circuits; the chromatographic column 14 is connected with the four-way valve 13 and the four-way valve 16 through gas circuits; the pulse discharge helium ionization detector 17 is connected with the four-way valve 16, the primary diluting device 1, the current limiter 2, the six-way valve 4 and the ten-way valve 11 through gas circuits.
The first-stage diluting device 1 is connected with the six-way valve 4 based on a three-way joint.
The four-way valve 13 is further connected with a pre-separation column based on a gas circuit, and the pre-separation column can prevent carbon dioxide from entering a rear chromatographic column 14.
The primary diluting device consists of an EPC control system, an air capillary column of 0.32mm multiplied by 30m, a capillary tee joint and a gas circuit connecting system and is used for diluting a gas sample.
The quantitative ring 3 is a quantitative ring which has the volume of 0.25mL and is treated by a passivation process.
The chromatographic column 6 adopts a DB-sulfurur-SCD capillary column or a Gaspro capillary column and is used for separating sulfur-containing gas components in sulfur hexafluoride electrical equipment.
The volume of the quantitative ring 9 and the quantitative ring 10 is 1mL, and the ten-way valve 11 is used for respectively conveying the gas samples in the two quantitative rings to a chromatographic column separation system.
The chromatographic column 12 adopts a CST pre-separation column, the chromatographic column 14 adopts a 13X packed column, and the chromatographic column 15 adopts a PQ packed column.
Specifically, the primary diluting device is connected with the port a of the six-way valve (4) through a three-way valve, and the standard sample or the sample enters the diluting device, is diluted according to a certain proportion and then enters the six-way valve (4) through the three-way valve. And the port a of the six-way valve (4) is connected with the port f, the port f is connected with the quantitative ring (3), the port b is connected with the port c, and the port b is an air outlet. By controlling the switch of the six-way valve (4), the gas sample enters the shunting/non-shunting sample inlet (5) through the quantitative ring, enters the chromatographic column for separation after being diluted again through the shunting/non-shunting sample inlet, and passes through the four-way valve (7) after separation. The port a in the four-way valve (7) is connected with the port b, the port c is connected with the port d, the switch of the four-way valve (7) is controlled, and SF is separated6The sulfur chemiluminescence detector (8) is switched off, and SF is fed through the b port6Discharge, reduce SF6Influence on the results of the detection of the sulfur-containing gas components.
Specifically, the primary dilution device (1) in the sulfur chemiluminescence detection unit (A) mainly comprises an EPC control system, an air capillary column of 0.32mm multiplied by 30m, a capillary tee joint and a gas circuit connection system, and is mainly used for diluting a gas sample. The quantitative ring (3) adopts a quantitative ring which has the volume of 0.25mL and is processed by a passivation process, the six-way valve (4) can transmit a gas sample to a chromatographic column separation system, the shunt/non-shunt sample inlet (5) can be used for secondary dilution, the chromatographic column (6) adopts a DB-sulfurr-SCD capillary column or a Gaspro capillary column and is used for separating sulfur-containing gas components in sulfur hexafluoride electrical equipment, and the four-way valve (7) mainly plays a role in separating SF6The gas is discharged to reduce sulfur-containing gas component, namely sulfuryl fluoride (SO)2F2) Thionyl fluoride (SOF)2) Hydrogen sulfide (H)2S), sulfur dioxide (SO)2) Carbonyl sulfide (COS), carbon disulfide (CS)2) And the sensitivity of the sulfur-containing gas components is improved under the influence of the detection result of the sulfur-containing gas components. Chemiluminescence detection of sulfurThe detector (8) is mainly used for detecting sulfur-containing gas components, the response of the sulfur chemiluminescence detector to sulfur elements is equimolar linear response, the sensitivity is high (less than 0.5pg S/sec), and the linearity is wide (more than 1 multiplied by 10)-4) And is not interfered by most sample matrixes and has no quenching effect.
Specifically, the pulse discharge helium ionization detection unit can detect hydrogen (H) in sulfur hexafluoride2) Oxygen (O)2) Nitrogen (N)2) Carbon monoxide (CO), methane (CH)4) Carbon tetrafluoride (CF)4) Carbon dioxide (CO)2) Hexafluoroethane (C)2F6) Octafluoropropane (C)3F8)。
Specifically, the pulse discharge helium ionization detection unit (B) mainly comprises quantitative rings (9, 10), a ten-way valve (11), chromatographic columns (12, 14, 15), four-way valves (13, 16) and a pulse discharge helium ionization detector (17). In the ten-way valve (11), the port a is connected with the port b, the port c is connected with the port d, the port e is connected with the port f, the port g is connected with the port h, and the port i is connected with the port j. Firstly, a sample enters a quantitative ring (9) through an i port and a j port in a ten-way valve (11), the switch of the ten-way valve (11) is controlled, the sample enters a CST pre-separation column (12), and meanwhile, after the ten-way valve (11) is switched, the sample of a second path also enters a quantitative ring (10). And after passing through the CST pre-separation column (12), the first path of sample passes through a four-way valve (13), carbon dioxide (CO2) components are discharged, an a port of the four-way valve (13) is connected with a d port, a b port of the four-way valve (13) is connected with a c port, the four-way valve (13) is controlled to be opened and closed, and the first path of sample enters a 13X packing column for separation and then enters a four-way valve (16). And the port a of the four-way valve (16) is connected with the port b, the port b is connected with the port c, and the separated sample enters a pulse discharge helium ionization detector (17) under the condition of not switching the four-way valve (16). And after the second path of sample comes out of the quantitative loop (10), the second path of sample directly enters a PQ packed column for separation, the separated sample enters a four-way valve (16), and the four-way valve (16) is controlled to be switched on and off, so that the sample also enters a pulse discharge helium ionization detector (17) for detection.
The volume of quantitative rings (9, 10) in the pulse discharge helium ionization detection unit (B) is 1mL, and a ten-way valve (11) can respectively convey gas samples in the two quantitative rings to a chromatographic column separation system
The chromatographic column (12) is a CST pre-separation column with the caliber of 1/8 inches and the length of 0.5m, and mainly used for adsorbing carbon dioxide (CO)2) Without allowing carbon dioxide (CO)2) Into a chromatographic column (14).
The chromatographic column (14) was a 13X packed column having a size of 1/8 inches in bore and a length of 1.6m, and was primarily used to separate hydrogen (H)2) Oxygen (O)2) Nitrogen (N)2) Carbon monoxide (CO), methane (CH)4) Carbon tetrafluoride (CF)4) And the like.
The chromatographic column (15) is a PQ packed column with a diameter of 1/8 inches and a length of 7.8m, and is mainly used for separating carbon dioxide (CO)2) Hexafluoroethane (C)2F6) Octafluoropropane (C)3F8) And the like.
By using a combination of a Sulfur Chemiluminescence Detector (SCD) and a Pulsed Discharge Helium Ionization Detector (PDHID), the sulfur chemiluminescence detector has equimolar linear response to the response of sulfur-containing compounds, high sensitivity (< 0.5pg S/sec), and wide linearity (> 1 × 10)-4) The sulfur chemiluminescence detection unit can detect sulfuryl fluoride (SO) in sulfur hexafluoride without the interference of most sample matrixes and quenching effect and the like2F2) Thionyl fluoride (SOF)2) Hydrogen sulfide (H)2S), sulfur dioxide (SO)2) Carbonyl sulfide (COS), carbon disulfide (CS)2) The gas components are equal; a Pulse Discharge Helium Ionization Detector (PDHID) is a high-sensitivity nondestructive detector with a response linear range of 10 to organic substances5The minimum detection limit can be as low as ppb level
Detection application one
Using sulfur hexafluoride (SF)6) Sulfuryl fluoride (SO) of (1)2F2) Thionyl fluoride (SOF)2) Hydrogen sulfide (H)2S), sulfur dioxide (SO)2) The example of the mixture detection is illustrated: the DB-Sulfur SCD capillary column is adopted to separate the four components in the Sulfur hexafluoride gas; by hand feedIn the sample mode, different standard gases are mixed (mixed with 0.1mL of sulfur hexafluoride pure gas), and the mixture enters an SCD detector for detection after components are separated by a separation system. The column temperature was 35 ℃ and held for 10 min. The second-stage flow ratio is 20:1, the flow rate of a chromatographic column is 0.7mL/min, and the sample injection amount is 0.1 mL. The detector base temperature was 250 deg.C and the detector burner tip temperature was 800 deg.C. Sulfuryl fluoride (SO) appears in qualitative time of 6.481min, 6.714min, 7.233min and 7.893min2F2) Thionyl fluoride (SOF)2) Hydrogen sulfide (H)2S), sulfur dioxide (SO)2) And the chromatographic peaks of the four components are obtained, and the separation effect is good. The chromatographic peak is shown in figure 2.
Detection application two
Using sulfur hexafluoride (SF)6) The detection example of the carbonyl sulfide (COS) mixed gas is illustrated as follows: carbonyl sulfide (COS) in sulfur hexafluoride gas is detected by using a Gaspro capillary column, components are separated by a separation system in a manual sample introduction mode, and then the components enter an SCD detector for detection. The column temperature was 40 ℃ and held for 15 min. The secondary dilution (split ratio) was set to 50:1, column flow 2mL/min, sample volume 0.1mL, detector base temperature 200 ℃ and detector burner temperature 800 ℃. Carbonyl sulfide (COS) peaks appeared at qualitative times of 13.161min, respectively. The chromatographic peak is shown in FIG. 3.
Detection application three
Using sulfur hexafluoride (SF)6) Carbon disulfide (CS) in (1)2) The example of the mixture detection is illustrated: detection of Carbonyl Sulfide (CS) in sulfur hexafluoride gas using Gaspro capillary column2) And separating the components by a separation system in a manual sample introduction mode, and then detecting the components by an SCD detector. And (3) adopting a programmed heating mode, wherein the column temperature is initially 70 ℃, the temperature is kept for 8.35min, the heating rate is 15 ℃/min, and the temperature is kept for 8min after being heated to 160 ℃. The secondary dilution (split ratio) was set to 20:1, column flow 2mL/min, sample volume 0.1mL, detector base temperature 200 ℃ and detector burner temperature 800 ℃. Carbonyl Sulfide (CS) appeared at qualitative time of 14.676min2) Chromatographic peak. The chromatographic peak is shown in FIG. 4.
Detection application four
Using sulfur hexafluoride (SF)6) Hydrogen (H) in (1)2) Oxygen (O)2) Nitrogen (N)2) Carbon monoxide (CO), methane (CH)4) Carbon tetrafluoride (CF)4) Carbon dioxide (CO)2) Hexafluoroethane (C)2F6) Octafluoropropane (C)3F8) The example of the mixture detection is illustrated: the method comprises the steps of detecting the nine gas components by adopting a CST pre-separation column, a 13X packed column and a PQ packed column, separating the components by a separation system in an automatic valve sample injection mode, and then detecting the components by using a PDHID detector. The constant temperature mode is adopted, the column temperature is 50 ℃, and the temperature is kept for 30 min. The secondary dilution (split ratio) was set to 20:1, chromatographic column flow 0.7mL/min, quantitative loop sample volume 0.1mL, detector temperature 180 ℃. Hydrogen (H) appears at qualitative time of 0.461min, 0.880min, 1.199min, 2.2min, 2.440min, 3.027min, 3.215min, 5.211min, 6.816min, 23.387min2) Oxygen (O)2) Nitrogen (N)2) Carbon monoxide (CO), methane (CH)4) Carbon tetrafluoride (CF)4) Carbon dioxide (CO)2) Hexafluoroethane (C)2F6) Octafluoropropane (C)3F8) Chromatographic peak and good separation effect. The chromatographic peak is shown in FIG. 5.
The system for detecting gas components in sulfur hexafluoride electrical equipment provided by the embodiment of the present invention is described in detail above, and the principle and the embodiment of the present invention are explained in the present specification by using specific examples, and the description of the above embodiments is only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (8)
1. A system for detecting a gaseous component in sulfur hexafluoride electrical equipment, said system comprising: a sulfur chemiluminescence detection unit and a pulsed discharge helium ionization detection unit, wherein:
the sulfur chemiluminescence monitoring unit comprises: the device comprises a primary diluting device 1, a current limiter 2, a quantitative ring 3, a six-way valve 4, a split/non-split sample inlet 5, a chromatographic column 6, a four-way valve 7 and a sulfur chemiluminescence detector 8;
the pulse discharge helium ionization detection unit comprises a quantitative ring 9, a quantitative ring 10, a ten-way valve 11, a chromatographic column 12, a chromatographic column 14, a chromatographic column 15, a four-way valve 13, a four-way valve 16 and a pulse discharge helium ionization detector 17;
the primary diluting device 1 is connected with the six-way valve 4, the current limiter 2, the ten-way valve 11, the pulse discharge helium ionization detector 17 and the four-way valve 13 through gas circuits;
the flow restrictor 2 is connected with the four-way valve 7, the primary diluting device 1, the flow restrictor 2, the ten-way valve 11, the pulse discharge helium ionization detector 17 and the four-way valve 13 through gas circuits;
the quantitative ring 3 is connected to the six-way valve 4 through a gas path;
the flow dividing/non-flow dividing sample inlet 5 is connected with the four-way valve 7 and the chromatographic column 6 through a gas circuit;
the chromatographic column 6 is connected with the four-way valve 7 through a gas circuit, and the sulfur chemiluminescence detector 8 is connected with the four-way valve 7 through a gas circuit;
the chromatographic column 12 is connected with the ten-way valve 11 and the four-way valve 13 through gas circuits;
the chromatographic column 15 is connected with the ten-way valve 11 and the four-way valve 16 through gas circuits;
the chromatographic column 14 is connected with the four-way valve 13 and the four-way valve 16 through gas circuits;
the pulse discharge helium ionization detector 17 is connected with the four-way valve 16, the primary diluting device 1, the current limiter 2, the six-way valve 4 and the ten-way valve 11 through gas circuits.
2. The system for detecting the gas composition in sulfur hexafluoride electrical equipment as claimed in claim 1, wherein said primary dilution means 1 is connected to said six-way valve 4 based on a three-way joint.
3. The system for detecting the gas composition in sulfur hexafluoride electrical equipment of claim 2, wherein said four-way valve 13 is further connected to a pre-separation column based on a gas path.
4. The system for detecting the gaseous component in sulfur hexafluoride electrical equipment of claim 3, wherein said primary dilution unit comprises an EPC control system, a 0.32mm x 30m empty capillary column, a capillary tee, and a gas circuit connection system for diluting the gaseous sample.
5. The system for detecting the gas composition in sulfur hexafluoride electrical equipment of claim 4, wherein said quantitative ring 3 is a passivation quantitative ring having a volume of 0.25 mL.
6. The system for detecting the gas composition in sulfur hexafluoride electrical equipment of claim 5, wherein said chromatographic column 6 uses a DB-sulfurr-SCD capillary column or a Gaspro capillary column for separation of sulfur containing gas composition in sulfur hexafluoride electrical equipment.
7. The system for detecting the gas composition in sulfur hexafluoride electrical equipment of claim 6, wherein said quantitative ring 9 and said quantitative ring 10 have a volume of 1mL, and said ten-way valve 11 is used to separately transfer the gas samples in the two quantitative rings to the chromatographic column separation system.
8. The system for detecting the gas composition in sulfur hexafluoride electrical equipment of claim 7, wherein said chromatographic column 12 is a CST pre-separation column, said chromatographic column 14 is a 13X packed column, and said chromatographic column 15 is a PQ packed column.
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|---|---|---|---|
| CN202011092183.6A CN112362766A (en) | 2020-10-13 | 2020-10-13 | System for detecting gas components in sulfur hexafluoride electrical equipment |
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